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Radiation damage of liquid electrolyte during focused X-ray beam photoelectron spectroscopy



Christopher M. Arble, Hongxuan Gou, Evgheni Strelcov, Brian D. Hoskins, Patrick Zeller, Matteo Amati, Luca Gregoratti, Andrei A. Kolmakov


Ambient pressure X-ray photoelectron spectroscopy (APXPS) has become an effective tool to interrogate chemical states at surfaces relevant to real operational conditions. Herein we employ a graphene-capped microvolume array sample platform for scanning photoelectron microscopy (SPEM) of liquid-solid electrochemical interfaces using traditional ultra-high vacuum systems. By using the graphene membrane as a working electrode within this setup, we were able to probe the electronic structure of a model electroplating system in operando conditions within the first few nanometers of the electrode/liquid electrolyte interface. We observed that intense X-ray irradiation may affect the chemistry at the liquid-solid interface due to solvent radiolysis by primary radiation, photo- and secondary electrons. We recorded radiolytic products by photoemission spectroscopy and characterized their impact on the chemical speciation at the electrified solid-liquid interface. Three different exposure regimes were tested to elucidate the dependence of XPS radiolytic signatures of the dose rate. The observed effects highlight the need for a careful consideration of radiolytic processes during liquid phase XPS measurements to correctly interrupt experimental results and minimize artifacts
Surface Science
Created April 12, 2020, Updated June 18, 2020